Zinc sulfide nano material with chiral morphology and preparation method thereof

By combining inorganic compounds with chiral ligands and calcination, the method addresses the complexity and instability issues in chiral inorganic nano material synthesis, resulting in stable and controllable chiral zinc sulfide nanoparticles.

CN120309001APending Publication Date: 2025-07-15XI AN JIAOTONG UNIV
View PDF 0 Cites 1 Cited by

Patent Information

Application Number
CN202510391168.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-31
Publication Date
2025-07-15

AI Technical Summary

Technical Problem

The existing synthesis methods of chiral inorganic nanomaterials are complex, low efficiency, and limited chiral stability of materials, making it difficult to achieve accurate and controllable synthesis.

Method used

The co-precipitation method is used to combine chiral ligands and zinc salt solutions to prepare zinc sulfide nanomaterials with chiral morphology by calcining. The chiral ligands are used as morphological modifiers and chiral inducers in the synthesis of ZnS nanomaterials to form stable S-Zn bonds.

Benefits of technology

The preparation process is simple and low cost. The obtained zinc sulfide nanomaterial has high crystallinity and stability, and is suitable for the construction and regulation of chiral inorganic nanomaterials.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120309001A_ABST
    Figure CN120309001A_ABST
Patent Text Reader

Abstract

The invention discloses a zinc sulfide nano material with chiral morphology and a preparation method thereof, and the method comprises the following steps: 1, adding an alkali source solution into a chiral ligand aqueous solution, and carrying out ultrasonic treatment at 30 DEG C to obtain a chiral ligand reaction precursor solution; 2, adding a zinc salt solution into the chiral ligand reaction precursor solution, and stirring to obtain a mixed turbid solution; 3, placing the mixed turbid liquid in a water bath kettle at the temperature of 15-50 DEG C, keeping the temperature for 3-30 minutes, separating out precipitates, washing and freeze-drying to obtain a zinc-chiral ligand complex nano material; and 4, transferring the zinc-chiral ligand complex nano-material to a quartz porcelain boat, putting the quartz porcelain boat into a tubular furnace, heating from room temperature to 300-700 DEG C at a heating rate of 1-5 DEG C / min in a protective atmosphere, calcining for 1-12 hours, and cooling to obtain the zinc sulfide nano-material with chiral morphology. The preparation method is simple, easy to control, low in cost and high in universality, and the prepared chiral zinc sulfide nano material has good crystallinity and stability.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to chiral nano-inorganic materials, and specifically to a zinc sulfide nano-material with a chiral morphology and a preparation method thereof. Background Art

[0002] Chirality refers to the property that an object cannot be completely superimposed with its mirror image through symmetry operations such as rotation and translation. Similar to human hands, although they have similar shapes, they cannot be completely overlapped. Chiral materials have received extensive attention due to the special physical and chemical properties endued by their asymmetric structures, and show unique advantages and application prospects especially in aspects such as polarized light regulation, optical detection, molecular recognition, and spin selectivity.

[0003] In recent years, chiral inorganic nano-materials have shown broad application prospects in frontier fields such as chiral sensing, spintronic devices, asymmetric catalysis, photoelectrocatalysis, and biomedicine due to their excellent chemical stability and broadband optical response ability, and have become a research hotspot of chiral materials. However, at present, chiral inorganic nano-materials are still in the initial stage of development, and the current means for constructing and regulating their chiral structures are not yet mature, making it difficult to achieve precise and controllable synthesis of chiral structures, which greatly limits their further development and practical applications. Therefore, exploring the synthesis of stable and tunable chiral inorganic nano-materials not only helps to promote their feasibility in practical applications, but also is conducive to deeply understanding their chiral origin and related action mechanisms.

[0004] At present, the synthesis of chiral inorganic nano-materials is gradually developing. For example: the chiral ligand adsorption and transfer chiral strategy connects surface chiral ligands with inorganic nano-materials to transfer chirality from organic molecules to inorganic materials; the organic / inorganic chiral template method uses a pre-synthesized chiral template to guide the directional assembly of inorganic nano-particles, and removes the template by means such as dissolution or calcination to obtain a chiral inorganic nano-structure. Although these methods can achieve the construction of chiral inorganic nano-materials to a certain extent, they generally have problems such as complex preparation processes, low efficiency, and limited chiral stability of the prepared materials. Summary of the Invention

[0005] Aiming at the deficiencies of the existing technology, the purpose of the present invention is to provide a zinc sulfide nano-material with a chiral morphology and a preparation method thereof, which not only has a simple, easy-to-control, low-cost, and highly universal preparation method, but also the prepared chiral zinc sulfide nano-material has good crystallinity and stability.

[0006] To achieve the above purpose, the present invention adopts the following technical solutions to implement:

[0007] A preparation method of a zinc sulfide nano-material with a chiral morphology, comprising the following steps:

[0008] Step 1: Add 0.5 - 20 mL of a base source solution with a concentration of 0.01 - 2.5 mol / L to 1 - 500 mL of an aqueous chiral ligand solution with a concentration of 0.01 - 0.5 mol / L, and perform ultrasonic dispersion at 30 °C to obtain a precursor solution of the chiral ligand reaction.

[0009] The aqueous chiral ligand solution is a sulfur-containing amino acid solution or a sulfur-free amino acid solution.

[0010] Step 2: Add the precursor solution of the chiral ligand reaction to 15 - 500 mL of a zinc salt solution with a concentration of 0.01 - 0.5 mol / L and stir to obtain a mixed turbid solution.

[0011] Step 3: Place the mixed turbid solution in a water bath at 15 - 50 °C, keep it warm for 3 - 30 min, centrifuge to separate the precipitate, wash and freeze-dry it in sequence to obtain a zinc-chiral ligand complex nanomaterial.

[0012] Step 4: Prepare a zinc sulfide nanomaterial with a chiral morphology

[0013] When the chiral ligand solution is a sulfur-containing amino acid solution, transfer the zinc-chiral ligand complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat in a tube furnace, and under a protective atmosphere, heat it from room temperature to 300 - 700 °C at a heating rate of 1 - 5 °C / min, calcine for 1 - 12 h, and after cooling, obtain a zinc sulfide nanomaterial with a chiral morphology.

[0014] When the chiral ligand solution is a sulfur-free amino acid solution, place the zinc-chiral ligand complex nanomaterial at one end of a quartz porcelain boat, place 1 - 100 mg of sulfur powder at the other end of the quartz porcelain boat, place the quartz porcelain boat in a tube furnace, and under a protective atmosphere, heat it from room temperature to 300 - 700 °C at a heating rate of 1 - 5 °C / min, calcine for 1 - 12 h, and after cooling, obtain a zinc sulfide nanomaterial with a chiral morphology.

[0015] Further, the base source solution in Step 1 is a sodium hydroxide solution, a potassium hydroxide solution, or an ammonia water solution.

[0016] Further, the sulfur-containing amino acid solution in Step 1 is prepared from a sulfur-containing amino acid and pure water, where: the sulfur-containing amino acid is L-cystine, D-cystine, L-cysteine, D-cysteine, L-homocysteine, or D-homocysteine.

[0017] Further, the sulfur-free amino acid solution in Step 1 is prepared from a sulfur-free amino acid and pure water, where: the sulfur-free amino acid is L-tartaric acid, D-tartaric acid, L-proline, D-proline, L-aspartic acid, D-aspartic acid, L-threonine, D-threonine, L-alanine, D-alanine, L-valine, or D-valine.

[0018] Further, the time for ultrasonic dispersion in Step 1 is 30 min.

[0019] Further, the zinc salt solution in Step 2 is prepared by the following method: adding zinc salt into pure water, and performing ultrasonic dispersion at 30 °C for 15 min to obtain the zinc salt solution;

[0020] The zinc salt is zinc chloride, zinc nitrate, zinc acetate or zinc bromide.

[0021] Further, the stirring time in Step 2 is 30 min.

[0022] Further, the washing in Step 3 is to perform centrifugal cross-washing with deionized water and ethanol for 3 to 5 times.

[0023] Further, the freeze-drying in Step 3 is performed at -80 to -40 °C for at least 12 h.

[0024] A zinc sulfide nanomaterial with a chiral morphology.

[0025] Compared with the prior art, the present invention has the following technical effects:

[0026] 1), The present invention combines an inorganic compound and a chiral ligand. First, a chiral complex precursor is synthesized by a coprecipitation method, and then the chiral complex precursor is calcined to obtain a zinc sulfide nanomaterial with a chiral morphology. The organic ligand serves as both a morphology modifier and a chiral inducer in the synthesis process of the ZnS nanomaterial. Groups such as -NH2 and -COOH in its molecular structure can have a strong coordination effect with Zn 2 +, and relying on the point chirality characteristics inside cystine, the precursor gradually forms a twisted structure during the ordered stacking process. Moreover, during the calcination process, most of the carbon and oxygen in the organic ligand molecules are removed to form stable S-Zn bonds, thereby successfully constructing a zinc sulfide (ZnS) nanomaterial with a specific morphology.

[0027] 2), The present invention has the advantages of easy realization of reaction conditions, simple reaction process, low cost and high generality. Moreover, the prepared chiral ZnS nanomaterial has high crystallinity and stability, which is of great significance for constructing and regulating new chiral inorganic nanomaterials. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is the XRD pattern of the zinc sulfide nanomaterial with a chiral morphology synthesized in Examples 1 to 6 of the present invention;

[0029] Figure 2Circular dichroism spectra of zinc sulfide nanomaterials with chiral morphology synthesized in Example 1 and Example 7 of the present invention, and achiral zinc sulfide nanomaterials synthesized in Comparative Example 1;

[0030] Figure 3 Transmission electron microscope image of the zinc sulfide nanomaterial with chiral morphology synthesized in Example 1 of the present invention;

[0031] Figure 4 Circular dichroism spectra of zinc sulfide nanomaterials with chiral morphology synthesized in Examples 1 to 6 of the present invention. Detailed implementation manners

[0032] The following further elaborates on the specific content of the present invention in conjunction with examples.

[0033] In Examples 1 to 9, the sulfur-containing amino acids selected, in addition to L-cystine, D-cystine, D-cysteine, or L-homocysteine, may also be L-cysteine or D-homocysteine.

[0034] In Examples 10 to 12, the sulfur-free amino acids selected, in addition to L-tartaric acid, L-proline, or D-tartaric acid, may also be D-proline, L-aspartic acid, D-aspartic acid, L-threonine, D-threonine, L-alanine, D-alanine, L-valine, or D-valine.

[0035] Example 1

[0036] Step 1: Add D-cystine to pure water to prepare a D-cystine solution with a concentration of 0.1 mol / L. Add 1.5 mL of a sodium hydroxide solution with a concentration of 2.5 mol / L to 13.5 mL of the D-cystine solution, and ultrasonically disperse it at 30 °C for 30 min to obtain a D-cystine reaction precursor solution;

[0037] Step 2: Add zinc acetate to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc acetate solution with a concentration of 0.1 mol / L;

[0038] Step 3: Add 15 mL of the zinc acetate solution to the D-cystine reaction precursor solution and stir for 30 min to obtain a mixed turbid solution;

[0039] Step 4: Place the mixed turbid solution in a water bath at 30 °C, keep it warm for 15 min, centrifuge it at a speed of 8000 r / min for 5 min, separate the precipitate, wash it 4 times by centrifugal cross-washing with deionized water and ethanol, and freeze-dry it at -80 °C for 12 h to obtain a zinc-D-cystine complex nanomaterial;

[0040] Step 5: Transfer the zinc-D-cysteine complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat into a tube furnace, at 20 °C, purge the tube furnace with nitrogen for 30 min to remove the oxygen inside the tube furnace. Then, with a heating rate of 5 °C / min, heat from room temperature to 450 °C, calcine for 4 h, and after cooling, obtain zinc sulfide nanomaterials with chiral morphology.

[0041] Example 2

[0042] The only difference from Example 1 is that the calcination temperature in Step 5 is 550 °C and the calcination time is 8 h.

[0043] Example 3

[0044] The only difference from Example 1 is that the calcination temperature in Step 5 is 500 °C and the calcination time is 8 h.

[0045] Example 4

[0046] The only difference from Example 1 is that the calcination temperature in Step 5 is 500 °C and the calcination time is 4 h.

[0047] Example 5

[0048] The only difference from Example 1 is that the calcination temperature in Step 5 is 450 °C and the calcination time is 8 h.

[0049] Example 6

[0050] The only difference from Example 1 is that the calcination temperature in Step 5 is 400 °C and the calcination time is 4 h.

[0051] Example 7

[0052] Step 1: Add L-cysteine to pure water to prepare an L-cysteine solution with a concentration of 0.01 mol / L. Add 20 mL of a potassium hydroxide solution with a concentration of 0.01 mol / L to 500 mL of the L-cysteine solution, and ultrasonically disperse for 30 min at 30 °C to obtain an L-cysteine reaction precursor solution;

[0053] Step 2: Add zinc acetate to pure water and ultrasonically disperse for 15 min at 30 °C to obtain a zinc acetate solution with a concentration of 0.01 mol / L;

[0054] Step 3: Add 500 mL of the zinc acetate solution to the L-cysteine reaction precursor solution and stir for 30 min to obtain a mixed turbid solution;

[0055] Step 4: Place the mixed turbid solution in a water bath at 15°C, keep it warm for 30 min, centrifuge at a speed of 6000 r / min for 15 min to separate the precipitate, wash it 3 times by centrifugation with deionized water and ethanol alternately, and freeze-dry it at -40°C for 12 h to obtain the zinc-L-cysteine complex nanomaterial;

[0056] Step 5: Transfer the zinc-L-cysteine complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat in a tube furnace, purge the tube furnace with nitrogen at 20°C for 30 min to remove the oxygen inside the tube furnace, then heat it from room temperature to 300°C at a heating rate of 1°C / min and calcine for 12 h. After cooling, obtain the zinc sulfide nanomaterial with chiral morphology.

[0057] Example 8

[0058] Step 1: Add L-homocysteine to pure water to prepare an L-homocysteine solution with a concentration of 0.13 mol / L. Add 15 mL of potassium hydroxide solution with a concentration of 0.63 mol / L to 385 mL of the L-homocysteine solution, and ultrasonically disperse it at 30°C for 30 min to obtain the L-homocysteine reaction precursor solution;

[0059] Step 2: Add zinc chloride to pure water and ultrasonically disperse it at 30°C for 15 min to obtain a zinc chloride solution with a concentration of 0.5 mol / L;

[0060] Step 3: Add 50 mL of the zinc chloride solution to the L-homocysteine reaction precursor solution and stir for 30 min to obtain a mixed turbid solution;

[0061] Step 4: Place the mixed turbid solution in a water bath at 20°C, keep it warm for 20 min, centrifuge at a speed of 6000 r / min for 10 min to separate the precipitate, wash it 5 times by centrifugation with deionized water and ethanol alternately, and freeze-dry it at -60°C for 12 h to obtain the zinc-L-homocysteine complex nanomaterial;

[0062] Step 5: Transfer the zinc-L-homocysteine complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat in a tube furnace, purge the tube furnace with nitrogen at 20°C for 30 min to remove the oxygen inside the tube furnace, then heat it from room temperature to 400°C at a heating rate of 4°C / min and calcine for 8 h. After cooling, obtain the zinc sulfide nanomaterial with chiral morphology.

[0063] Example 9

[0064] Step 1: Add D-cysteine to pure water to prepare a D-cysteine solution with a concentration of 0.25 mol / L. Add 10 mL of ammonia water with a concentration of 1.25 mol / L to 250 mL of the D-cysteine solution, and ultrasonically disperse it at 30 °C for 30 min to obtain a D-cysteine reaction precursor solution;

[0065] Step 2: Add zinc nitrate to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc nitrate solution with a concentration of 0.25 mol / L;

[0066] Step 3: Add 250 mL of the zinc nitrate solution to the D-cysteine reaction precursor solution and stir for 30 min to obtain a mixed turbid solution;

[0067] Step 4: Place the mixed turbid solution in a water bath at 25 °C, keep it warm for 15 min, centrifuge it at a speed of 9000 r / min for 8 min, separate the precipitate, wash it 4 times by centrifugal cross-washing with deionized water and ethanol, and freeze-dry it at -80 °C for 12 h to obtain a zinc-D-cysteine complex nanomaterial;

[0068] Step 5: Transfer the zinc-D-cysteine complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat in a tubular furnace, purge the tubular furnace with nitrogen at 20 °C for 30 min to remove the oxygen inside the tubular furnace, then heat it from room temperature to 600 °C at a heating rate of 3 °C / min and calcine it for 10 h. After cooling, a zinc sulfide nanomaterial with a chiral morphology is obtained.

[0069] Example 10

[0070] Step 1: Add L-tartaric acid to pure water to prepare an L-tartaric acid solution with a concentration of 0.37 mol / L. Add 5 mL of potassium hydroxide with a concentration of 1.8 mol / L to 126 mL of the L-tartaric acid solution, and ultrasonically disperse it at 30 °C for 30 min to obtain an L-tartaric acid reaction precursor solution;

[0071] Step 2: Add zinc bromide to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc bromide solution with a concentration of 0.37 mol / L;

[0072] Step 3: Add 126 mL of the zinc bromide solution to the L-tartaric acid reaction precursor solution and stir for 30 min to obtain a mixed turbid solution;

[0073] Step 4: Place the mixed turbid solution in a water bath at 40 °C, keep it warm for 10 min, centrifuge it at a speed of 10000 r / min for 3 min, separate the precipitate, wash it 5 times by centrifugal cross-washing with deionized water and ethanol, and freeze-dry it at -60 °C for 12 h to obtain a zinc-L-tartaric acid complex nanomaterial;

[0074] Step 5: Transfer the zinc-L-tartrate complex nanomaterial to one end of a quartz boat. Place 1 mg of sulfur powder at the other end of the quartz boat. Put the quartz boat into a tube furnace. At 20 °C, purge the tube furnace with nitrogen for 30 min to remove the oxygen inside the tube furnace. Then, heat it from room temperature to 700 °C at a heating rate of 2 °C / min and calcine for 6 h. After cooling, zinc sulfide nanomaterials with chiral morphology are obtained.

[0075] Example 11

[0076] Step 1: Add D-tartaric acid to pure water to prepare a D-tartaric acid solution with a concentration of 0.5 mol / L. Add 0.5 mL of ammonia water with a concentration of 2.1 mol / L to 1 mL of the D-tartaric acid solution. Ultrasonically disperse it at 30 °C for 30 min to obtain a D-tartaric acid reaction precursor solution.

[0077] Step 2: Add zinc acetate to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc acetate solution with a concentration of 0.01 mol / L.

[0078] Step 3: Add 50 mL of the zinc acetate solution to the D-tartaric acid reaction precursor solution and stir for 30 min to obtain a mixed turbid solution.

[0079] Step 4: Place the mixed turbid solution in a water bath at 50 °C, keep it warm for 3 min, centrifuge at a speed of 10000 r / min for 5 min to separate the precipitate, wash it 3 times by centrifugation with deionized water and ethanol alternately, and freeze-dry it at -40 °C for 12 h to obtain zinc-D-tartrate complex nanomaterials.

[0080] Step 5: Transfer the zinc-D-tartrate complex nanomaterial to one end of a quartz boat. Place 50 mg of sulfur powder at the other end of the quartz boat. Put the quartz boat into a tube furnace. At 20 °C, purge the tube furnace with nitrogen for 30 min to remove the oxygen inside the tube furnace. Then, heat it from room temperature to 550 °C at a heating rate of 2 °C / min and calcine for 8 h. After cooling, zinc sulfide nanomaterials with chiral morphology are obtained.

[0081] Example 12

[0082] Step 1: Add L-proline to pure water to prepare an L-proline solution with a concentration of 0.2 mol / L. Add 8 mL of sodium hydroxide solution with a concentration of 0.1 mol / L to 335 mL of the L-proline solution. Ultrasonically disperse it at 30 °C for 30 min to obtain an L-proline reaction precursor solution.

[0083] Step 2: Add zinc acetate to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc acetate solution with a concentration of 0.13 mol / L.

[0084] Step 3: Add 258 mL of zinc acetate solution to the L-proline reaction precursor solution, and stir for 30 min to obtain a mixed turbid solution.

[0085] Step 4: Place the mixed turbid solution in a water bath at 35 °C, keep it warm for 25 min, centrifuge at a speed of 8000 r / min for 10 min, separate the precipitate, wash it 3 times by centrifugation with deionized water and ethanol alternately, and freeze-dry it at -50 °C for 12 h to obtain zinc-L-proline complex nanomaterials.

[0086] Step 5: Transfer the zinc-L-proline complex nanomaterials to one end of a quartz porcelain boat, place 100 mg of sulfur powder at the other end of the quartz porcelain boat, put the quartz porcelain boat into a tube furnace, purge the tube furnace with nitrogen at 20 °C for 30 min to remove the oxygen inside the tube furnace, then heat it from room temperature to 500 °C at a heating rate of 5 °C / min, calcine for 4 h, and after cooling, obtain zinc sulfide nanomaterials with chiral morphology.

[0087] Comparative Example 1

[0088] Step 1: Add DL-cystine to pure water to prepare a DL-cystine solution with a concentration of 0.1 mol / L. Add 1.5 mL of sodium hydroxide solution with a concentration of 2.5 mol / L to 13.5 mL of the DL-cystine solution, and ultrasonically disperse it at 30 °C for 30 min to obtain a DL-cystine reaction precursor solution.

[0089] Step 2: Add zinc acetate to pure water and ultrasonically disperse it at 30 °C for 15 min to obtain a zinc acetate solution with a concentration of 0.1 mol / L.

[0090] Step 3: Add 15 mL of zinc acetate solution to the DL-cystine reaction precursor solution, and stir for 30 min to obtain a mixed turbid solution.

[0091] Step 4: Place the mixed turbid solution in a water bath at 30 °C, keep it warm for 15 min, centrifuge at a speed of 8000 r / min for 5 min, separate the precipitate, wash it 4 times by centrifugation with deionized water and ethanol alternately, and freeze-dry it at -80 °C for 12 h to obtain zinc-DL-cystine complex nanomaterials.

[0092] Step 5: Transfer the zinc-DL-cystine complex nanomaterials to a quartz porcelain boat, put the quartz porcelain boat into a tube furnace, purge the tube furnace with nitrogen at 20 °C for 30 min to remove the oxygen inside the tube furnace, then heat it from room temperature to 450 °C at a heating rate of 5 °C / min, calcine for 4 h, and after cooling, obtain achiral zinc sulfide nanomaterials.

[0093] Figure 1XRD patterns of the zinc sulfide nanomaterials with chiral morphologies synthesized in Examples 1 to 6 are shown. It can be seen that the characteristic peaks of zinc sulfide (PDF#05-0566) exist in the prepared zinc sulfide nanomaterials with chiral morphologies, and the characteristic peaks are relatively sharp, indicating that the prepared zinc sulfide nanomaterials have good crystallinity. In addition, as the calcination temperature increases and the calcination time prolongs, the characteristic peaks of zinc oxide gradually appear.

[0094] Figure 2 Circular dichroism spectra of the zinc sulfide nanomaterials with chiral morphologies synthesized in Example 1 and Example 7 and the achiral zinc sulfide nanomaterials synthesized in Comparative Example 1 are shown. It can be seen that the CD curves of the zinc sulfide nanomaterials with chiral morphologies synthesized in Example 1 and Example 7 are basically mirror-symmetric, while the CD curve of the achiral zinc sulfide nanomaterials synthesized in Comparative Example 1 basically remains at 0, indicating that it does not have chiral characteristics.

[0095] Figure 3 Transmission electron microscopy images of the zinc sulfide nanomaterials with chiral morphologies synthesized in Example 1 are shown. It can be seen that it is composed of small nanoparticles, providing a larger active surface area. Moreover, the overall morphology is distorted, attributed to the generation of chiral morphology.

[0096] Figure 4 Circular dichroism spectra of the zinc sulfide nanomaterials with chiral morphologies synthesized in Examples 1 to 6 are shown. It can be seen that the CD curves of the zinc sulfide nanomaterials synthesized in Examples 1 to 6 are basically mirror-symmetric, proving that chiral zinc sulfide nanomaterials are synthesized in Examples 1 to 6.

Claims

1. A preparation method of a zinc sulfide nanomaterial with a chiral morphology, characterized in that, It includes the following steps: Step 1: Add 0.5 - 20 mL of an alkali source solution with a concentration of 0.01 - 2.5 mol / L to 1 - 500 mL of an aqueous solution of a chiral ligand with a concentration of 0.01 - 0.5 mol / L, and perform ultrasonic dispersion at 30 °C to obtain a reaction precursor solution of the chiral ligand. The aqueous solution of the chiral ligand is a sulfur-containing amino acid solution or a sulfur-free amino acid solution. Step 2: Add 15 - 500 mL of a zinc salt solution with a concentration of 0.01 - 0.5 mol / L to the reaction precursor solution of the chiral ligand, and stir to obtain a mixed turbid solution. Step 3: Place the mixed turbid solution in a water bath at 15 - 50 °C, keep it warm for 3 - 30 min, centrifuge to separate the precipitate, wash it successively and freeze-dry it to obtain a zinc-chiral ligand complex nanomaterial. Step 4: Prepare a zinc sulfide nanomaterial with a chiral morphology When the chiral ligand solution is a sulfur-containing amino acid solution, transfer the zinc-chiral ligand complex nanomaterial to a quartz porcelain boat, place the quartz porcelain boat in a tube furnace, under a protective atmosphere, with a heating rate of 1 - 5 °C / min, heat from room temperature to 300 - 700 °C, calcine for 1 - 12 h, and after cooling, obtain a zinc sulfide nanomaterial with a chiral morphology. When the chiral ligand solution is a sulfur-free amino acid solution, transfer the zinc-chiral ligand complex nanomaterial to one end of a quartz porcelain boat, place 1 - 100 mg of sulfur powder at the other end of the quartz porcelain boat, place the quartz porcelain boat in a tube furnace, under a protective atmosphere, with a heating rate of 1 - 5 °C / min, heat from room temperature to 300 - 700 °C, calcine for 1 - 12 h, and after cooling, obtain a zinc sulfide nanomaterial with a chiral morphology.

2. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The alkali source solution in Step 1 is a sodium hydroxide solution, a potassium hydroxide solution or ammonia water.

3. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The sulfur-containing amino acid solution in Step 1 is prepared from a sulfur-containing amino acid and pure water, where: the sulfur-containing amino acid is L-cystine, D-cystine, L-cysteine, D-cysteine, L-homocysteine or D-homocysteine.

4. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The sulfur-free amino acid solution in Step 1 is prepared from a sulfur-free amino acid and pure water, where: the sulfur-free amino acid is L-tartaric acid, D-tartaric acid, L-proline, D-proline, L-aspartic acid, D-aspartic acid, L-threonine, D-threonine, L-alanine, D-alanine, L-valine or D-valine.

5. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The time for ultrasonic dispersion in Step 1 is 30 min.

6. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The zinc salt solution in Step 2 is prepared by the following method: Add a zinc salt to pure water, and perform ultrasonic dispersion for 15 min at 30 °C to obtain a zinc salt solution. The zinc salt is zinc chloride, zinc nitrate, zinc acetate or zinc bromide.

7. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The stirring time in Step 2 is 30 min.

8. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, characterized in that, The washing in Step 3 is to perform centrifugal cross-washing with deionized water and ethanol 3 - 5 times.

9. The preparation method of the zinc sulfide nanomaterial with chiral morphology according to claim 1, wherein, The freeze-drying in Step 3 is at -80 - -40 °C for at least 12 h.

10. A zinc sulfide nanomaterial with a chiral morphology prepared by the method according to any one of claims 1 - 9.

Citation Information

Cited By

  • Efficient synthesis method of ephedrine hydrochloride

    CN121085799A